CN106573281A - Process for wood torrefaction, and construction material produced therefrom - Google Patents
Process for wood torrefaction, and construction material produced therefrom Download PDFInfo
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- CN106573281A CN106573281A CN201580019546.4A CN201580019546A CN106573281A CN 106573281 A CN106573281 A CN 106573281A CN 201580019546 A CN201580019546 A CN 201580019546A CN 106573281 A CN106573281 A CN 106573281A
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- kpas
- charring process
- cellulosic material
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- 238000000034 method Methods 0.000 title claims abstract description 107
- 230000008569 process Effects 0.000 title claims description 85
- 239000002023 wood Substances 0.000 title abstract description 11
- 239000004035 construction material Substances 0.000 title description 5
- 239000000463 material Substances 0.000 claims description 59
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 238000003763 carbonization Methods 0.000 claims description 31
- 239000007789 gas Substances 0.000 claims description 30
- 238000002425 crystallisation Methods 0.000 claims description 25
- 230000008025 crystallization Effects 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229920002488 Hemicellulose Polymers 0.000 claims description 16
- 229920005610 lignin Polymers 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 238000000354 decomposition reaction Methods 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 9
- 229910052756 noble gas Inorganic materials 0.000 claims description 9
- 150000002835 noble gases Chemical class 0.000 claims description 9
- 229920002678 cellulose Polymers 0.000 claims description 7
- 239000001913 cellulose Substances 0.000 claims description 7
- CVTZKFWZDBJAHE-UHFFFAOYSA-N [N].N Chemical compound [N].N CVTZKFWZDBJAHE-UHFFFAOYSA-N 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000010583 slow cooling Methods 0.000 claims description 5
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 abstract description 3
- 230000006835 compression Effects 0.000 abstract 2
- 238000007906 compression Methods 0.000 abstract 2
- 230000001351 cycling effect Effects 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229910052743 krypton Inorganic materials 0.000 description 3
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052754 neon Inorganic materials 0.000 description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007799 cork Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011121 hardwood Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 241000208140 Acer Species 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000007954 hypoxia Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004899 motility Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/0085—Thermal treatments, i.e. involving chemical modification of wood at temperatures well over 100°C
- B27K5/009—Thermal treatments, i.e. involving chemical modification of wood at temperatures well over 100°C using a well-defined temperature schedule
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Environmental & Geological Engineering (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Paper (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The present disclosure includes methods for enhancing hardness and dimensional stability of a wood element. In one embodiment, the method includes placing the wood element in a compression assembly set to a compression temperature between about 120 DEG C and about 230 DEG C in a temperature cycling matter and cooling it slowly under low atmospheric pressure.
Description
Cross reference related application
The application advocates the priority of No. 62/069,921 earlier patent application in the U.S., applies as on October 29th, 2014, aforementioned
The description of application is integrally joined to this by quoting.
Background technology
Carbonization is a kind of cracking liquid wax, tar and dust and extracts the gentle mode of its volatile ingredient.These compounds
It is all harmful to environment thus need to be destroyed according to specific flow process or be reclaimed.The invention discloses how one kind controls compound
Waste and they are changed into the production technology of recovering energy source safely.
It is well known that carbonization is a kind of technique for making timber more robust.Simply the surface of burn wood can just make its more resistant to
With.The key of the present invention is to improve lumber quality and ruggedness by improving carbonization process.
Carbonization need to carry out heat wood with very high temperature in the dry kiln of controlled gas pressure and hypoxia, generally from 190 DEG C to 240
℃.Time and temperature are depending on by the wood type of carbonization and desired target and color.Carbonization needs three steps：It is dry
Dry, heat treatment and cooling.Pre-drying process is needed using traditional kiln drier, as convention, accounts for mixing in water vapour content
Initial humidity is reduced between 6% and 10% on certain particular value on the basis of the ratio of the total air content of thing.It is dried then
Humidity is reduced to into 0% further.Timber is placed on one by controlling injection steam to realize temperature gradually in the final step
In the room of reduction.The humidity of product increases between 3% and 6%, and this is, in order to give timber natural motility, to contribute to adjusting
Section timber stability, promotes the more preferable quality of production.
Existing method is difficult to control to, and is lack of consistency by the possible difference of the property of charred wood, and final generation need not
The waste wanted and cost.The technique that the present invention proposes the reliability and product quality of novel an increased production.
In carbonization, various gases can be reacted, such as carbon monoxide, carbon dioxide, various organic compound, water and other
Inorganic compound.One aspect of the present invention is combusting carbon monoxide and organic vapor and uses its heat for dry and carbonization
Some heat energy are provided.Noble gases obviously potentially include steam as such as nitrogen and/or other noble gases.Cellulose carbonization
Product, irreducible water more specifically and volatilization raw material, in closing, the inertia of a volatile material for allowing capture
System in implement.
The content of the invention
The present invention is specifically, there is provided a kind of charring process based on cellulosic material, including：
1) cellulose carries out first time crystallization at a temperature of about 210 DEG C to about 240 DEG C, and about 10 minutes time is to about
45 minutes, pressure was of about 25.4 kPas to about 101.4 kPas；
2) lignose material is decomposed at a temperature of 170 DEG C to 200 DEG C, about 15 minutes time by 35 minutes, lazy
In the environment of the pressure of property gas is of about 50.8 kPas to about 101.4 kPas, there are 0.05-0.1% ammonias；；
3) cellulosic material carries out second crystallization at a temperature of about 205 DEG C to about 230 DEG C, and about 15 minutes time arrived
90 minutes, about 50.8 kPas to about 101.4 kPas of pressure, period is under noble gases with the strong of increase cellulosic material
Degree；
4) at a temperature of about 50 DEG C to about 95 DEG C, the time is of about 60 minutes to greatly to the water balance of cellulosic material
About 120 minutes, pressure was for about 10.2 kPas to about 75.2 kPas, and cellulosic material is preferentially back to room temperature (about 25 DEG C) and normally
Under atmospheric pressure (about 101.325 kPas).
Crystallization for the first time can be carried out in ozone, nitrogen or a noble gases.
Crystallization for the first time can be carried out in nitrogen.
Crystallization for the first time can be at 230 DEG C.
Crystallization for the first time can last about 15 minutes.
First subcrystalline air pressure can be at about 50.7 kPas (0.5atm).
Lignin decomposition can be at 180 DEG C.
Lignin decomposition can be about 20 minutes.
Lignin decomposition can be about 101.4 kPas (about 1atm).
Lignin decomposes can be carried out under an inert gas.
Noble gases can be nitrogen.
Lignin decomposes the 0.05-0.1% ammonia that can further take presence.
Lignin decomposes can be carried out under nitrogen-ammonia gas.
Second crystallization can be at about 210 DEG C to 215 DEG C.
Sustainable 30 minutes to 50 minutes are crystallized for the second time.
Water balance step can be at about 81.1 kPa 0.8 (atm) and be about 101.4 kPas (about 1atm).
Water balance step may be carried out in atmospheric humidity about 50%.
Charring process may further include gas and sour extraction step, before first time crystallizes.
Gas and sour extraction step may be about 120 DEG C.
Gaseous acid extraction step is probably 90 minutes to 120 minutes.
Gas and sour extraction step may be about 101.4 kPas (about 1atm)
Carbonization process may further constitute hemicellulose switch process, crystallize through second.
Hemicellulose switch process may be about 195 DEG C.
Hemicellulose switch process may about 15 minutes.
Hemicellulose switch process may be about 101.4 kPas of atm) (about 1atm).
Hemicellulose switch process can be carried out under nitrogen-ammonia gas.
Charring process may further include Slow cooling step after crystallizing at second, in about 1 minute at about 210 DEG C,
About 91.3 kPas (0.9atm).
The step of charring process may further include carbonization, which is after hemicellulose switch process.
Carbonization may be about 120 DEG C.
Carbonization is probably about 45 minutes.
Carbonization is probably about 101.4 kPas (about 1atm).
Charring process may further include compacting step, and which is after carbonization.
Compacting step may be about 180 DEG C.
Compacting step is probably about 15 minutes.
Compacting step is probably about 91.3 kPas (0.9atm).
Following term definition.
" cellulosic material " generally refers to timber, this be probably cork (such as coniferals) or hardwood (such as Oak Tree, maple, etc.).
" specific humidity " refers on quality base, and vapor is represented with % relative to the ratio of the shared mixture of air total amount.
" percentage ratio " is when the percentage ratio of air is referred to, it is meant that ratio of the component relative to air total amount.
During selected embodiment of the features and advantages of the invention prize described in detail by following, such as illustrate in appended numeral,
Can be clearer.As will be realized, the modification made in different aspect by disclosed scheme and claim, without departing from
Protection domain.Therefore, drawing and description should be considered illustrative, rather than as restricted and limiting of its scope.
Description of the drawings
In conjunction with accompanying drawing, from the following detailed description further disclose the present invention the characteristics of and advantage, wherein:
Fig. 1 illustrates the artwork of the carbonization of prior art.
Fig. 2 illustrates the artwork of the carbonization of the present invention.Red line represents mean temperature, and top level line represents 180 °C, solid line generation
The temperature of table cellulosic material (wood), other (different) lines represent the temperature of instrument.Heating period from about O DEG C to 180 DEG C,
Carbonization stage starts at 180 DEG C to maximum temperature is reached, and cooling stage starts to stop process from maximum temperature.
The flow chart that Fig. 3 illustrates the technique of an embodiment of the present invention.Specific humidity, shows as being worth the ratio mixing of %
The vapor content of the total air of thing is on the basis of quality.
The flow chart that Fig. 4 illustrates (A) and (B) technique of an embodiment of the present invention.(A) illustrate the basic mistake of the present invention
Journey, while the optional step that (B) may be introduced in illustrating present invention process.
Specific embodiment
The charring process of some cellulosic materials will be disclosed in embodiment.The technique of the present invention is one non-for needed for making acquisition
The inflammable heat absorption and exothermic reaction that correct degree of carbonization can be reached as the cellulosic material (wood) of construction material of drying
Complex set.Existing charring process can be with reference to the acid (mainly acetic acid and formic acid) for being released from cellulose decomposition (degeneration), meeting
Cause mechanical suitable material more fragile.
The present invention overcomes these problems, optimizes the hydrolysis of wood polysaccharose such as by controlling the pH value in environment (acid to neutrality),
And it and most sufficient charring process window (temperature, gas, pH value, time and pressure) are combined into maximally effective to obtain
The residual mass percentage ratio of preservative-treated timber, and with required performance (resistance to water, enough grindabilities, few fragility, highest
Mechanical strength (process/cutting), the susceptibility for covering and protecting and slower degradation process).
Referring to Fig. 4 A, according to one embodiment, accelerate and improve different cultivars timber there is provided a charring process 100
Carbonization condition, including cork and hardwood, and the final cellulosic material product of the purpose built based on improving.The present invention
Charring process 100 be related to different process sequences to improve the product applied in final building structure.The technique of the present invention
The temperature that As time goes on final products are used is adjusted between 120 DEG C to 240 DEG C, including gas with various condition, is increased
Reduce free radical while stiffened is spent as far as possible.It is related to sequence of events in the technique of the present invention, from ozone, nitrogen or rare gas
Dry heat under (such as argon) gas starts, and is followed by vacuum drying, and temperature and humidity declines process.In order to prepare construction material
And do not go to burn material, the control of temperature control and air is most important for carbonization level.The present invention technique it is main excellent
Gesture is the decomposition that can control wood-cellulose to keep the sufficient mechanical strength needed for construction application, and the final product of control
The color of product.
According to one embodiment of charring process 100, the cellulosic material of crystallization 10 for the first time may be subject to can be at 210 DEG C and to be arrived
240 DEG C, or from 210 DEG C to 235 DEG C, or from 210 DEG C to 230 DEG C, or from 210 DEG C to 225 DEG C, or from 210 DEG C to 220 DEG C, or
From 210 DEG C to 215 DEG C, or about 215 DEG C to 240 DEG C, or from 215 DEG C to 235 DEG C, or from 215 DEG C to 230 DEG C, or from 215 DEG C to
225 DEG C, or from 215 DEG C to 220 DEG C, or about 220 DEG C to 240 DEG C, or from 220 DEG C to 235 DEG C, or from 220 DEG C to 230 DEG C, or
From 220 DEG C to 225 DEG C, or about 225 DEG C to 240 DEG C, or from 225 DEG C to 235 DEG C, or from 225 DEG C to 230 DEG C, or about 230 DEG C are arrived
240 DEG C, or from 230 DEG C to 235 DEG C, or, about 235 DEG C to 240 DEG C, preferably at 230 DEG C.Crystallization for the first time may be about 10
About 45 minutes minutes, or from about 40 minutes about 10 minutes, or from about 10 minutes by 35 minutes, or from about 10 points
Clock by 30 minutes, or from about 10 minutes by 25 minutes, or from about 10 minutes, 20 minutes, or from about 10 minutes to 15 points
Clock, or from 15 minutes by 45 minutes, or from about 15 minutes by about 40 minutes, or from about 15 minutes by 35 minutes, or from
About 15 minutes by 30 minutes, or from about 15 minutes by 25 minutes, or from about 15 minutes by 20 minutes, or from 20 minutes to
45 minutes, or from about 20 minutes by about 40 minutes, or from about 20 minutes by 35 minutes, or from about 20 minutes to 30 points
Clock, or from about 20 minutes by 25 minutes, or from 25 minutes by 45 minutes, or from about 25 minutes by about 40 minutes, or from about
25 minutes by 35 minutes, or from about 25 minutes by 30 minutes, or from 30 minutes by 45 minutes, or from about 30 minutes to about 40
Minute, or from about 30 minutes to 35 minutes, from 35 minutes by 45 minutes, or from about 40 minutes about 35 minutes, Huo Zhecong
40 minutes to 45 minutes, preferably at 15 minutes.
The performed pressure of crystallization 10 is in about 25.4 kPas to about 101.4 kPas for the first time, or from about 25.4 kPas to about
91.3 kPas, or from about 25.4 kPas to about 81.1 kPas, or from about 25.4 kPas to about 76.1 kPas, or from about 25.4 kPas
To about 71 kPas, or from about 25.4 kPas to about 60.8 kPas, or from about 25.4 kPas to about 50.7 kPas, or from about 25.4 thousand
Handkerchief to about 40.6 kPas, or from about 25.4 kPas to about 33.8 kPas, or from about 33.8 kPas to about 101.4 kPas, or from about
33.8 kPas to about 91.3 kPas, or from about 33.8 kPas to about 81.1 kPas, or from about 33.8 kPas to about 76.1 kPas, or
From about 33.8 kPas to about 71 kPas, or from about 33.8 kPas to about 60.8 kPas, or from about
33.8 kPas to about 50.7 kPas, or from about 33.8 kPas to about 40.6 kPas, or from about 40.6 kPas to about 101.4 thousand
Handkerchief, or from about 40.6 kPas about 91.3 kPas, or from about 40.6 kPas to about 40.6 kPas, or from about 40.6 kPas to about 76.1
KPa, or from about 40.6 kPas to about 71 kPas, or from about 40.6 kPas to about 60.8 kPas, or from about 40.6 kPas to about
50.7 kPas, or from about 50.7 kPas to about 101.4 kPas, or from about 50.7 kPas to about 91.3 kPas, or from about 50.7 thousand
Handkerchief to about 81.1 kPas, or from about 50.7 kPas to about 76.1 kPas, or from 50.7 kPas to about 71 kPas, or from about 50.7 thousand
Handkerchief to about 60.8 kPas, or from about 60.8 kPas to about 101.4 kPas, or from about 60.8 kPas to about 91.3 kPas, or from about
60.8 kPas to about 81.1 kPas, or from about 60.8 kPas to about 76.1 kPas, or from about 60.8 kPas to about 71 kPas, or from
About 71 kPas to about 101.4 kPas, or from about 71 kPas to about 91.3 kPas, or from 71 kPas to about 81.1 kPas, or
From 71 kPas to about 76.1 kPas, or from about 76.1 kPas to about 101.4 kPas, or from about 76.1 kPas to about 91.3 kPas,
Or from about 76.1 kPas to about 81.1 kPas, or from about 81.1 kPas to about 101.4 kPas, or from about 81.1 kPas to about 91.3
KPa, or from about 91.3 kPas to about 101.4 kPas, preferably at 50.7 kPas (0.5atm).
In embodiment, environment of the crystallization in ozone, nitrogen or rare (inertia) gas (such as helium, neon, argon, krypton, xenon) for the first time is performed
In carry out, preferred nitrogen.
This step may followed by lignin decomposition step 20, in 170 DEG C to 200 DEG C, or from 170 DEG C to 195 DEG C, or from
170 DEG C to 190 DEG C, or from 170 DEG C to 185 DEG C, or from 170 DEG C to 180 DEG C, or from 170 DEG C to 175 DEG C, or from 175 DEG C to
200 DEG C, or from 175 DEG C to 195 DEG C, or from 175 DEG C to 190 DEG C, or from 175 DEG C to 185 DEG C, or from 175 DEG C to 180 DEG C, or
From 180 DEG C to 200 DEG C, or from 180 DEG C to 195 DEG C, or from 180 DEG C to 190 DEG C, or from 180 DEG C to 185 DEG C, or from 185 DEG C to
200 DEG C, or from 185 DEG C to 195 DEG C, or from 185 DEG C to 190 DEG C, or from 190 DEG C to 200 DEG C, or from 190 DEG C to 195 DEG C, or
From about 195 DEG C to 200 DEG C, preferably 180 DEG C.Lignin decomposition step be probably about 15 minutes by 35 minutes, or from about
15 minutes by 30 minutes, or from about 15 minutes by 25 minutes, or from about 15 minutes by 20 minutes, or from about 20 minutes to
35 minutes, or from about 20 minutes by 30 minutes, or from about 20 minutes by 25 minutes, or from about 25 minutes by 35 minutes, or
From about 25 minutes by 30 minutes, or from about 30 minutes to 35 minutes, preferably 20 minutes.
Second step (lignin decomposes 20) may perform about 50.7 kPas to about 101.4 kPas of pressure, or about 50.7 kPas
To about 91.3 kPas, or about 50.7 kPas to about 81.1 kPas, or about 50.7 kPas to about 76.1 kPas, or about 50.7 kPas are arrived
About 71 kPas, or about 50.7 kPas to about 60.8 kPas, or from about 60.8 kPas to about 101.4 kPas, or about 60.8 kPas are arrived
About 91.3 kPas, or about 60.8 kPas to about 81.1 kPas, about 60.8 kPas to about 76.1 kPas, or 60.8 kPas arrive about 71,000
Handkerchief, or from about 71 kPas to about 101.4 kPas, or about 71 kPas to about 91.3 kPas, or about 71 kPas to about 81.1 kPas,
Or about 71 kPas to about 76.1 kPas, or from about 76.1 kPas to about 101.4 kPas, or about 76.1 kPas to about 91.3 kPas,
Or about 76.1 kPas to about 81.1 kPas, or from about 81.1 kPas to about 101.4 kPas, or about 81.1 kPas are arrived about 91.3 thousand
Handkerchief, or from about 91.3 kPas to about 101.4 kPas, preferably 101.4 kPas (1atm).
Second step (lignin decompose 20) may perform under an inert gas (as nitrogen or rare (inertia) gas (as helium,
Neon, argon, krypton, xenon) gas, preferred nitrogen), optional 0.05-0.1% ammonia.
The cellulosic material of second crystallization 30 may be subject to can be at about 205 DEG C to about 230 DEG C, or from about 205 DEG C to about
225 DEG C, or from about 205 DEG C to about 220 DEG C, or from about 205 DEG C to about 215 DEG C, or from about 205 DEG C to about 210 DEG C, or from about
210 DEG C to about 230 DEG C, or from about 210 DEG C to about 225 DEG C, or from about 210 DEG C to about 220 DEG C, or from about 210 DEG C to about 215
DEG C, or from about 215 DEG C to about 230 DEG C, or from about 215 DEG C to about 225 DEG C, or from about 215 DEG C to about 220 DEG C, or from about 220 DEG C
To about 230 DEG C, or from about 220 DEG C to about 225 DEG C, or from about 225 DEG C to about 230 DEG C, preferably from about 210 DEG C to about 210 DEG C, most preferably
It is about 215 DEG C.
Second crystallization 30 may be about 15 minutes by 90 minutes, or from about 15 minutes by 85 minutes, or from about 15 minutes
By 80 minutes, or from about 15 minutes by 75 minutes, or from about 15 minutes by 70 minutes, or from about 15 minutes to 65 points
Clock, or from about 15 minutes by 60 minutes, or from about 15 minutes by 55 minutes, or from about 15 minutes by about 50 minutes,
Or from about 15 minutes by 45 minutes, or from about 15 minutes by about 40 minutes, or from about 15 minutes by 35 minutes, or from
About 15 minutes by 30 minutes, or from about 15 minutes by 25 minutes, or from about 15 minutes by 20 minutes, or from about 20 points
Clock by 90 minutes, or from about 20 minutes by 85 minutes, or from about 20 minutes by 80 minutes, or from about 20 minutes to 75 points
Clock, or from about 20 minutes by 70 minutes, or from about 20 minutes by 65 minutes, or from about 20 minutes by 60 minutes, or from
About 20 minutes by 55 minutes, or from about 20 minutes by about 50 minutes, or from about 20 minutes by 45 minutes, or from big
About 20 minutes to about 40 minutes, or from about 20 minutes by 35 minutes, or from about 20 minutes by 30 minutes, or from about 20 points
Clock by 25 minutes, or from about 25 minutes by 90 minutes, or from about 25 minutes by 85 minutes, or from about 25 minutes by 80 minutes, or
From about 25 minutes by 75 minutes, or from about 25 minutes by 70 minutes, or from about 25 minutes by 65 minutes, or from about 25 minutes to 60
Minute, or from about 25 minutes by 55 minutes, or from about 25 minutes by about 50 minutes, or from about 25 minutes by 45 minutes, or from
About 40 minutes about 25 minutes, or from about 25 minutes by 35 minutes, or from about 25 minutes by 30 minutes, or from about 30 minutes to
90 minutes, or from about 30 minutes by 85 minutes, or from about 30 minutes by 80 minutes, or from about 30 minutes by 75 minutes,
Or from about 30 minutes by 70 minutes, or from about 30 minutes by 65 minutes, or from about 30 minutes by 60 minutes, or from about
30 minutes by 55 minutes, or from about 30 minutes by about 50 minutes, or from about 30 minutes by 45 minutes, or from about 30
Minute arrive about 40 minutes, or from about 30 minutes by 35 minutes, or from about 35 minutes by 90 minutes, or from about 35 minutes to
85 minutes, or from about 35 minutes by 80 minutes, or from about 35 minutes by 75 minutes, or from about 35 minutes by 70 minutes,
Or from about 35 minutes by 65 minutes, or from about 60 minutes 35 minutes, or from 55 minutes about 35 minutes, or from 35 minutes about 50 points
Clock, or from about 45 minutes about 35 minutes, or from about 40 minutes about 35 minutes, or from about 40 minutes by 90 minutes, or
From about 40 minutes by 85 minutes, or from about 40 minutes by 80 minutes, or from about 40 minutes by 75 minutes, or from about 40
Minute by 70 minutes, or from about 40 minutes by 65 minutes, or from about 40 minutes by 60 minutes, or from about 40 minutes to 55
Minute, or from about 40 minutes by about 50 minutes, or from about 40 minutes by 45 minutes, or from about 45 minutes to 90 points
Clock, or from about 45 minutes by 85 minutes, or from about 45 minutes by 80 minutes, or from about 45 minutes by 75 minutes, or from
About 45 minutes by 70 minutes, or from about 45 minutes by 65 minutes, or from about 45 minutes by 60 minutes, or from about 45 points
Clock by 55 minutes, or from about 45 minutes by about 50 minutes, or from about 50 minutes by 90 minutes, or from about 50 minutes to 85 points
Clock, or from about 50 minutes by 80 minutes, or from about 50 minutes by 75 minutes, or from about 50 minutes by 70 minutes, or from about 50 points
Clock by 65 minutes, or from about 60 minutes about 50 minutes, or from 55 minutes about 50 minutes, or from 55 minutes by 90 minutes, or from 55
Minute by 85 minutes, or from 55 minutes by 80 minutes, or from 55 minutes by 75 minutes, or from 55 minutes by 70 minutes, or from 55
Minute by 65 minutes, or from about 60 minutes about 55 minutes, or from about 60 minutes by 90 minutes, or from about 60 minutes by 85 minutes,
Or from about 60 minutes by 80 minutes, or from about 60 minutes by 75 minutes, or from about 60 minutes by 70 minutes, or from about 60 minutes to
65 minutes, or from about 65 minutes by 90 minutes, or from about 65 minutes by 85 minutes, or from about 65 minutes to 80 points
Clock, or from about 65 minutes by 75 minutes, or from about 65 minutes by 70 minutes, or from about 70 minutes by 90 minutes, or from
About 70 minutes by 85 minutes, or from about 70 minutes by 80 minutes, or from about 70 minutes by about 75 minutes, or from about 75
Minute by 90 minutes, or from about 75 minutes by 85 minutes, or from about 75 minutes by 80 minutes, or from about 80 minutes by 90 minutes,
Or from about 80 minutes by 85 minutes, or from about 85 minutes to 90 minutes, preferably 30 minutes to 50 minutes, be most preferably 30 minutes.
The execution of this step 30 is relevant with pressure, can be at about 50.7 kPas to 101.4 kPas, or about 50.7 kPas to about 91.3
KPa, or about 50.7 kPas to about 81.1 kPas, or about 50.7 kPas to about 76.1 kPas, or about 50.7 kPas to about 71,000
Handkerchief, or about 50.7 kPas to about 60.8 kPas, or from about 60.8 kPas to about 101.4 kPas, or about 60.8 kPas to about 91.3
KPa, or about 60.8 kPas to about 81.1 kPas, or about 60.8 kPas to about 76.1 kPas, or about 60.8 kPas to about 71,000
Handkerchief, or from 71 kPas to about 101.4 kPas, or about 71 kPas to about 91.3 kPas, or about 71 kPas to about 81.1 kPas, or about
71 kPas to about 76.1 kPas, or from about 76.1 kPas to about 101.4 kPas, or about 76.1 kPas to about 91.3 kPas, or about
76.1 kPas to about 81.1 kPas, or from about 81.1 kPas to about 101.4 kPas, or about 81.1 kPas to about 91.3 kPas, or
From about 91.3 kPas to about 101.4 kPas, preferably about 20.3 kPas (0.2atm), in order to increase the intensity of cellulosic material.
Step 30 can carry out (such as nitrogen or rare (inertia) gas (such as helium, neon, argon, krypton, xenon) gas) under an inert gas, preferably
Nitrogen, in order to increase the intensity of cellulosic material.
Cellulosic material and then experience in moisture balance step 40, be in about 50 DEG C to about 95 DEG C, or about 50 DEG C to about 90 DEG C,
Or about 50 DEG C to about 85 DEG C, or about 50 DEG C to about 80 DEG C, or about 50 DEG C to about 75 DEG C, or about 50 DEG C to about 70 DEG C, or about 50 DEG C
To about 65 DEG C, or about 50 DEG C to about 60 DEG C, or about 50 DEG C to about 55 DEG C, or from about 55 DEG C to about 95 DEG C, or about 55 DEG C to about 90
DEG C, or about 55 DEG C to about 85 DEG C, or about 55 DEG C to about 80 DEG C, or about 55 DEG C to about 75 DEG C, or about 55 DEG C to about 70 DEG C, or about 55
DEG C to about 65 DEG C, or about 55 DEG C to about 60 DEG C, or about 55 DEG C to about 55 DEG C, or from about 60 DEG C to about 95 DEG C, or about 60 DEG C to about
90 DEG C, or about 60 DEG C to about 85 DEG C, or about 60 DEG C to about 80 DEG C, or about 60 DEG C to about 75 DEG C, or about 60 DEG C to about 70 DEG C, or about
60 DEG C to about 65 DEG C, or from about 65 DEG C to about 95 DEG C, or about 65 DEG C to about 90 DEG C, or about 65 DEG C to about 85 DEG C, or about 65 DEG C extremely
About 80 DEG C, or about 65 DEG C to about 75 DEG C, or about 65 DEG C to about 70 DEG C, or from about 70 DEG C to about 95 DEG C, or about 70 DEG C to about 90 DEG C,
Or about 70 DEG C to about 85 DEG C, or about 70 DEG C to about 80 DEG C, or about 70 DEG C to about 75 DEG C, or from about 75 DEG C to about 95 DEG C, or about 75
DEG C to about 90 DEG C, or about 75 DEG C to about 85 DEG C, or about 75 DEG C to about 80 DEG C, or from about 80 DEG C to about 95 DEG C, or about 80 DEG C to about
90 DEG C, or about 80 DEG C to about 85 DEG C, or from about 85 ° DEG C to about 95 DEG C, or about 85 DEG C to about 90 DEG C, or from about 90 DEG C to about 95
DEG C, preferably 95 DEG C, third front cellulosic-based material be back to room temperature (about 25 DEG C) and normal atmosphere (An) (about 101.325 thousand
Handkerchief).
Water balance step 40 can be about 60 minutes to about 120 minutes, or from about 60 minutes to about 115 minutes, or from about
60 minutes to about 110 minutes, or from about 60 minutes to about 105 minutes, or from about 60 minutes to about 100 minutes, Huo Zhecong
About 60 minutes to about 95 minutes, or from about 60 minutes to about 90 minutes, or from about 60 minutes to about 85 minutes, or from about 60
Minute to about 80 minutes, or from about 60 minutes to about 75 minutes, or from about 60 minutes to about 70 minutes, or from about 60 points
Zhong Zhiyue 65 minutes, or from about 65 minutes to about 120 minutes, or from about 65 minutes to about 115 minutes, or about 65 minutes to about
110 minutes, or about 65 minutes to about 105 minutes, or about 65 minutes to about 100 minutes, or from about 65 minutes to about 95 minutes,
Or about 65 minutes to about 90 minutes, or about 65 minutes to about 85 minutes, or about 65 minutes to about 80 minutes, or about 65 minutes to about
75 minutes, or from about 65 minutes to about 70 minutes, or from about 70 minutes to about 120 minutes, or from about 70 minutes to about 115
Minute, or from about 70 minutes to about 110 minutes, or from about 70 minutes to about 105 minutes, or from about 70 minutes to about 100
Minute, or from about 70 minutes to about 95 minutes, or from about 70 minutes to about 90 minutes, or from about 70 minutes to about 85 points
Clock, or from about 70 minutes to about 80 minutes, or from about 70 minutes to about 75 minutes, or about 75 minutes to about 120 minutes or
About 75 minutes to about 115 minutes, or from about 75 minutes to about 110 minutes, or from about 75 minutes to about 105 minutes, or
From about 75 minutes to about 100 minutes, or from about 75 minutes to about 95 minutes, or from about 75 minutes to about 90 minutes, or about 75
Minute to about 85 minutes, or about 75 minutes to about 80 minutes, or from about 80 minutes to about 120 minutes, or from about 80 minutes
To about 115 minutes, or from about 80 minutes to about 110 minutes, or from about 80 minutes to about 105 minutes, or from about 80 minutes
To about 100 minutes, or from about 80 minutes to about 95 minutes, or from about 80 minutes to about 90 minutes, or from about 80 minutes
To about 85 minutes, or about 120 minutes about 85 minutes, or from about 85 minutes to about 115 minutes, or from about 85 minutes to about
110 minutes, or from about 85 minutes to about 105 minutes, or from about 85 minutes to about 100 minutes, or about 85 minutes arrive about 95
Minute, or from about 85 minutes to about 90 minutes, or from about 90 minutes to about 120 minutes, or from about 90 minutes to about 115
Minute, or from about 90 minutes to about 110 minutes, or from about 90 minutes by about 105 minutes, or from about 90 minutes to about
100 minutes, or from about 90 minutes to about 95 minutes, or from about 95 minutes to about 120 minutes, or from about 95 minutes to about
115 minutes, or about 110 minutes about 95 minutes, or from about 95 minutes to about 105 minutes, or from about 95 minutes to about 100
Minute, or from about 100 minutes to about 120 minutes, or from about 100 minutes to about 115 minutes, or from about 100 minutes about
110 minutes, or from about 100 minutes to about 105 minutes, or from about 105 minutes to about 120 minutes, or from about 105 minutes
To about 115 minutes, or from about 105 minutes to about 110 minutes, or from about about 120 minutes 110 minutes, or from about 110
Minute was to about 115 minutes, or from about 115 minutes to about 120 minutes, in preferably 60 minutes, cellulosic-based material was back to room
Before warm (about 25 DEG C) and normal atmosphere (An) (about 101.325 kPas).
Water balance step 40 can be carried out under stress, and with about 10.2 kPas to about 75.2 kPas, or about 10.2 kPas to about 71
KPa, or about 10.2 kPas to about 60.8 kPas, or about 10.2 kPas to about 50.7 kPas, or about 10.2 kPas to about 40.6 thousand
Handkerchief, or about 10.2 kPas to about 33.8 kPas, or about 10.2 kPas to about 25.4 kPas, or about 10.2 kPas to about 20.3 thousand
Handkerchief, or about 20.3 kPas to about 75.2 kPas, or about 20.3 kPas to about 71 kPas, or about 20.3 kPas to about 60.8 kPas,
Or about 20.3 kPas to about 50.7 kPas, or about 20.3 kPas to about 40.6 kPas, or about 20.3 kPas to about 33.8 kPas, or
About 20.3 kPas to about 25.4 kPas, or about 25.4 kPas to about 75.2 kPas, or about 25.4 kPas to about 71 kPas, or about
25.4 kPas to about 60.8 kPas, or about 25.4 kPas to about 50.7 kPas, or about 25.4 kPas to about 40.6 kPas, or about
25.4 kPas to about 33.8 kPas, or about 33.8 kPas to about 75.2 kPas, or about 33.8 kPas to about 71 kPas, or about 33.8
KPa to about 60.8 kPas, or about 33.8 kPas to about 50.7 kPas, or about 33.8 kPas to about 40.6 kPas, or about 40.6 thousand
Handkerchief to about 75.2 kPas, or about 40.6 kPas to about 71 kPas, or about 40.6 kPas to about 60.8 kPas, or about 40.6 kPas extremely
About 50.7 kPas, or about 50.7 kPas to about 75.2 kPas, or about 50.7 kPas to about 71 kPas, or about 50.7 kPas to about
60.8 kPas, or about 60.8 kPas to about 75.2 kPas, or about 60.8 kPas to about 71 kPas, or from about 71 kPas to about
75.2 kPas, preferably 50.7 kPas (0.5 atmospheric pressure), existing cellulosic-based material are back to room temperature (about 25 DEG C to) and just
Normal atmospheric pressure (about 101.325 kPas).According to one embodiment, gas balance step 40 is had about 40%, 50%, 60%,
Carry out under the gas of humidity, or about 40% to about 60%, or from about 40% to about 55%, or from about 40% to about 50%, or about
40% to about 45%, or from about 45% to about 60%, or from about 45% to about 55%, or about 45% to about 50%, %, or from
About 50% to about 60%, or from about 50% to about 55%, or about 55% to about 60%, preferably 50% humidity.
With reference now to Fig. 4 B, the technique of the present invention can include the several optional step of the characteristic of the material for further improving cellulose
Suddenly.
According to one embodiment, the method may include the optional gas and acid extraction step prior to first time crystallization 10
Rapid 12 this step can carry out for about 90 minutes to about 120 minutes, or from about 90 minutes to about 115 minutes, or from about 90
Minute to about 110 minutes, or from about 90 minutes to about 105 minutes, or from about 90 minutes to about 100 minutes, or from about
90 minutes to about 95 minutes, or from about 95 minutes to about 120 minutes, or from about 95 minutes to about 115 minutes, or from about
95 minutes to about 110 minutes, or from about 95 minutes to about 105 minutes, or from about 95 minutes to about 100 minutes, Huo Zhecong
About 100 minutes to about 120 minutes, or from about 100 minutes to about 115 minutes, or from about 100 minutes to about 110 minutes, or
Person from about 100 minutes to about 105 minutes, or from about 105 minutes to about 120 minutes, or from about 105 minutes to about 115 points
Clock, or from about 105 minutes to about 110 minutes, or from about 110 minutes to about 120 minutes, or from about 110 minutes to about
115 minutes, or from about 115 minutes to about 120 minutes.
Step 12 can be carried out at about 120 DEG C to about 140 DEG C, or from about 120 DEG C to about 135 DEG C, or from about 120 DEG C to about 130
DEG C, or from about 120 DEG C to about 125 DEG C, or from about 125 DEG C to about 140 DEG C, or from about 125 DEG C to about 135 DEG C, or from about 125 DEG C
To about 130 DEG C, or from about 130 DEG C to about 140 DEG C, or from about 130 DEG C to about 135 DEG C, or from about 135 DEG C to about 140 DEG C.
Step 12 can be carried out under about 70 kPas to about 110 kPas, or from about 70 kPas to about 105 kPas, or from about 70
KPa to about 100 kPas, or from about 70 kPas to about 95 kPas, or from about 70 kPas to about 90 kPas, or from about 70
KPa to about 85 kPas, or from about 70 kPas to about 80 kPas, or from about 70 kPas to about 75 kPas, or from about 75,000
Handkerchief to about 110 kPas, or from about 75 kPas to about 105 kPas, or from about 75 kPas to about 100 kPas, or from about 75
KPa to about 95 kPas, or from about 75 kPas to about 90 kPas, or from about 75 kPas to about 85 kPas, or from about 75,000
Handkerchief to about 80 kPas, or from about 80 kPas to about 110 kPas, or from about 80 kPas to about 105 kPas, or from about 80,000
Handkerchief to about 100 kPas, or from about 80 kPas to about 95 kPas, or from about 80 kPas to about 90 kPas, or from about 80,000
Handkerchief to about 85 kPas, or from about 85 kPas to about 110 kPas, or from about 85 kPas to about 105 kPas, or from about 85,000
Handkerchief to about 100 kPas, or from about 85 kPas to about 95 kPas, or from about 85 kPas to about 90 kPas, or from about 90,000
Handkerchief to about 110 kPas, or from about 90 kPas to about 105 kPas, or from about 90 kPas to about 100 kPas, or from about 90
KPa to about 95 kPas, or from about 95 kPas to about 110 kPas, or from about 95 kPas to about 105 kPas, or from about 95
KPa to about 100 kPas, or from about 100 kPas to about 110 kPas, or from about 100 kPas to about 105 kPas, Huo Zhecong
About 105 kPas to about 100 kPas, or from about 71 kPas to about 101.4 kPas, or about 71 kPas to about 91.3 kPas, or about
71 kPas to about 81.1 kPas, or about 71 kPas to about 76.1 kPas, or about 76.1 kPas to about 101.4 kPas, or about 76.1
KPa to about 91.3 kPas, or about 76.1 kPas to about 81.1 kPas, or about 81.1 kPas to about 101.4 kPas, or about 81.1
KPa to about 91.3 kPas, or about 91.3 kPas to about 101.4 handkerchiefs.
According to another embodiment, the method may include optional hemicellulose step of converting 32, and which can be at about 145 DEG C to about
Carry out at 195 DEG C, or from about 145 DEG C to about 190 DEG C, or from about 145 DEG C to about 185 DEG C, or from about 145 DEG C to about 180 DEG C, or
From about 145 DEG C to about 175 DEG C, or from about 145 DEG C to about 170 DEG C, or from about 145 DEG C to about 165 DEG C, or from about 145 DEG C to about
160 DEG C, or from about 145 DEG C to about 155 DEG C, or from about 145 DEG C to about 150 DEG C, or from about 150 DEG C to about 195 DEG C, or from about
150 DEG C to about 190 DEG C, or from about 150 DEG C to about 185 DEG C, or from about 150 DEG C to about 180 DEG C, or from about 150 DEG C to about 175 DEG C
C or for about 150 DEG C to about 110 DEG C, or from about 150 DEG C to about 165 DEG C, or from about 150 DEG C to about 160 DEG C, or from about 150 DEG C to
About 155 DEG C, or from about 155 DEG C to about 195 DEG C, or from about 155 DEG C to about 190 DEG C, or from about 155 DEG C to about 185 DEG C, or from about
155 DEG C to about 180 DEG C, or from about 155 DEG C to about 175 DEG C, or from about 155 DEG C to about 110 DEG C, or from about 155 DEG C to about 165
DEG C, or from about 155 DEG C to about 160 DEG C, or from about 160 DEG C to about 195 DEG C, or from about 160 DEG C to about 190 DEG C, or from about 160 DEG C
To about 185 DEG C, or from about 160 DEG C to about 180 DEG C, or from about 160 DEG C to about 175 DEG C, or from about 160 DEG C to about 110 DEG C, or from
About 160 DEG C to about 165 DEG C, or from about 165 DEG C to about 195 DEG C, or from about 165 DEG C to about 190 DEG C, or from about 165 DEG C to about 185
DEG C, or from about 165 DEG C to about 180 DEG C, or from about 165 DEG C to about 175 DEG C, or from about 165 DEG C to about 170 DEG C, or from about 170 DEG C
To about 195 DEG C of C, or from about 170 DEG C to about 190 DEG C, or from about 170 DEG C to about 185 DEG C, or from about 170 DEG C to about 180 DEG C, or
From about 170 DEG C to about 175 DEG C, or from about 175 DEG C to about 195 DEG C, or from about 175 DEG C to about 190 DEG C, or from about 175 DEG C to about
185 DEG C, or from about 175 DEG C to about 180 DEG C, or from about 180 DEG C to about 195 DEG C, or from about 180 DEG C to about 190 DEG C, or from about
180 DEG C to about 185 DEG C, or from about 185 DEG C to about 195 DEG C, or from about 185 DEG C to about 190 DEG C, or from about 190 DEG C to about 195
DEG C, preferably 195 DEG C.
Step 32 can carry out about 10 minutes～about 25 minutes, or about 10 minutes to about 20 minutes, or about 10 minutes to about 15 minutes
The conversion of optional hemicellulose, or from about 15 minutes to about 25 minutes, or about 15 minutes to about 20 minutes, or about 20 minutes extremely
About 25 minutes, preferably 15 minutes.
Optional hemicellulose step of converting 32 can be carried out under 70 kPas to about 110 kPas, or from about 70 kPas to about 105
KPa, or from about 70 kPas to about 100 kPas, or from about 70 kPas to about 95 kPas, or from about 70 kPas to about 90,000
Handkerchief, or from about 70 kPas to about 85 kPas, or from about 70 kPas to about 80 kPas, or from about 70 kPas to about 75,000
Handkerchief, or from about 75 kPas to about 110 kPas, or from about 75 kPas to about 105 kPas, or from about 75 kPas to about 100,000
Handkerchief, or from about 75 kPas to about 95 kPas, or from about 75 kPas to about 90 kPas, or from about 75 kPas to about 85,000
Handkerchief, or from about 75 kPas to about 80 kPas, or from about 80 kPas to about 110 kPas, or from about 80 kPas to about 105,000
Handkerchief, or from about 80 kPas to about 100 kPas, or from about 80 kPas to about 95 kPas, or from about 80 kPas to about 90 kPas,
Or from about 80 kPas to about 85 kPas, or from about 85 kPas to about 110 kPas, or from about 85 kPas to about 105 kPas,
Or from about 85 kPas to about 100 kPas, or from about 85 kPas to about 95 kPas, or from about 85 kPas to about 90 kPas, or
Person from about 90 kPas to about 110 kPas, or from about 90 kPas to about 105 kPas, or from about 90 kPas to about 100 kPas,
Or from about 90 kPas to about 95 kPas, or from about 95 kPas to about 110 kPas, or from about 95 kPas to about 105 kPas, or
Person from about 95 kPas to about 100 kPas, or from about 100 kPas to about 110 kPas, or from about 100 kPas to about 105 kPas,
Or from about 105 kPas to about 100 kPas, or from about 71 kPas to about 101.4 kPas, or about 71 kPas to about 91.3 thousand
Handkerchief, or about 71 kPas to about 81.1 kPas, or about 71 kPas to about 76.1 kPas, or about 76.1 kPas to about 101.4 kPas, or
About 76.1 kPas to about 91.3 kPas, or about 76.1 kPas to about 81.1 kPas, or about 81.1 kPas to about 101.4 kPas, or
About 81.1 kPas about 91.3 kPas, or about 91.3 kPas to about 101.4 kPas, preferably 101.4 kPas.Hemicellulose conversion step
Rapid 32 can be carried out under nitrogen-ammonia gas, and for example in the nitrogen comprising about 0.05 to 0.1% ammonia, (relative concentration is relative to total
Gas).
According to another embodiment, the method for the present invention can include Slow cooling initial step 34, after first time crystallization 30,
About 210 DEG C about 1 minute, under about 91.3 kPas (0.9 atmospheric pressure).
According to another embodiment, it is other carbonization 34 that the method for the present invention can replace Slow cooling initial step,
This is carried out at about 110 DEG C～about 130 DEG C, or about 110 DEG C to about 125 DEG C, or about 110 DEG C to about 120 DEG C, or about 110 DEG C
To about 115 DEG C, or about 115 DEG C to about 130 DEG C, or about 115 DEG C to about 125 DEG C, or about 115 DEG C to about 120 DEG C, or about 120 DEG C
To about 130 DEG C, or about 120 DEG C to about 125 DEG C, or about 125 DEG C to about 130 DEG C, preferably 120 DEG C.Carbonization 34 can be carried out
About 30 minutes to about 50 minutes, or about 30 minutes to about 45 minutes or about 30 minutes to about 40 minutes or about 30 minutes to about 35 points
Zhong Congyue be for about 35 minutes to about 50 minutes, or from about 35 minutes to about 45 minutes or about 35 minutes to about 40 minutes or about
40 minutes to about 50 minutes, or about 40 minutes to about 45 minutes, or about 45 minutes to about 50 minutes, preferably 45 minutes, about
91.3 to about 110 kPas, or about 91.3 to about 101.4 kPas, preferably 101.4 kPas.
Additionally, according in another embodiment, can and then in pressing step 36, at about 175 DEG C to about after carbonization 34
Carry out at 190 DEG C, or from about 175 DEG C to about 185 DEG C, or from about 175 DEG C to about 180 DEG C, or from about 180 DEG C to about 190 DEG C, or
From about 180 DEG C to about 185 DEG C, or from about 185 DEG C to about 190 DEG C, preferably 180 DEG C, at about 10 minutes to about 20 minutes, or about
10 minutes to about 15 minutes, or about 15 minutes to about 20 minutes, preferably 15 minutes, at about 81.1 kPas to about 101.4 kPas, or
About 81.1 kPas to about 91.3 kPas, or about 91.3 kPas (0.9 atmospheric pressure) to about 101.4 kPas (1 atmospheric pressure).The present invention will
The present invention is understood with more being had a thorough knowledge of by the following example, its objective is to make it possible to be more easily understood rather than
Limit its scope.
Example 1
Exemplary processes #1
According to one embodiment, the method for the present invention be one for control the decomposition of natural organic polymeric materials and the temperature made and when
Between circulation, wherein give the characteristic of construction material or element needed for which, such as each layer of moisture of the material of cellulose,
Stability, ruggedness, intensity, toughness, weatherability, coating character and glue performance.
According to one embodiment of present invention, carbonizing apparatus, circulates according to specified temp and time, and alternate gas or vacuum
Injection.Such as following table describes the technique by realizing the structural material step for providing optimization in single device：
Table 1- exemplary process #1
Example 2
Exemplary process #2
According to another embodiment, the method for the present invention can relate to the following circulation in carbonizing apparatus：
Table 2- example flows #2
Example 3
Exemplary processes #3
According to another embodiment, the minimum of the method for the present invention must step processing cellulosic-based material and suitably repair
The Nomenclature Composition and Structure of Complexes of the material for changing is：
Table 3- exemplary process #3
In other steps proposed by the present invention by according to expected purposes limiting the desirable characteristics of timber.
Example 4
Circulation technology under controlled air
Fig. 3 is described in the flow chart for specifying the technique change of controlled air in kiln.Injection noble gases and/or ammonia are (to neutralize
Acid) durability of timber has been significantly increased.
Embodiments of the present invention are described above in conjunction with drawings and Examples, the structure that embodiment is provided is not constituted to this
Bright restriction, according to the adjustment for needing to make in protection domain.
Claims (42)
1. a kind of charring process based on cellulosic material, it is characterised in that include：
1）Cellulose carries out first time crystallization at a temperature of about 210 °C to about 240 °C, and about 10 minutes time is to about
45 minutes, pressure was of about 25.4 kPas to about 101.4 kPas；
2) lignose material is decomposed at a temperature of 170 °C to 200 °C, about 15 minutes time by 35 minutes, lazy
In the environment of the pressure of property gas is of about 50.8 kPas to about 101.4 kPas；
3) cellulosic material carries out second crystallization at a temperature of about 205 °C to about 230 °C, and about 15 minutes time arrived
90 minutes, about 50.8 kPas to about 101.4 kPas of pressure, period is under noble gases with increase cellulosic material
Intensity;
4) at a temperature of about 50 °C to about 95 °C, the time is of about 60 minutes to greatly to the water balance of cellulosic material
About 120 minutes, pressure was for about 10.2 kPas to about 75.2 kPas, and cellulosic material is preferentially back to room temperature (about 25 °C) and normally
Under atmospheric pressure (about 101.325 kPas).
2. charring process according to claim 1, it is characterised in that：Crystallization can be in ozone, nitrogen or an inertia for the first time
Carry out in gas.
3. charring process according to claim 2, it is characterised in that：Crystallization for the first time can be carried out in nitrogen.
4. charring process according to claim 1, it is characterised in that：Crystallization for the first time can be at 230 °C.
5. according to arbitrary described charring process in Claims 1-4, it is characterised in that：Crystallization for the first time can last about 15 points
Clock.
6. according to arbitrary described a kind of charring process in claim 1 to 5, it is characterised in that：First subcrystalline air pressure can
In about 50.7 kPas (0.5 atm).
7. according to arbitrary described a kind of charring process in claim 1 to 6, it is characterised in that：Lignin decomposition can be at about
180°C。
8. according to arbitrary described a kind of charring process in claim 1 to 7, it is characterised in that：Lignin decomposition can be about 20
Minute.
9. according to arbitrary described a kind of charring process in claim 1 to 8, it is characterised in that：Lignin decomposition can be about
101.4 kPas (about 1 atm).
10. according to arbitrary described charring process in claim 1 to 9, it is characterised in that：Lignin decomposes can be in noble gases
Under carry out.
11. charring process according to claim 10, it is characterised in that：Noble gases are nitrogen.
12. according to arbitrary described charring process in claim 1 to 10, it is characterised in that：Lignin decomposes and further can account for
With 0.05-0.1% ammonia for existing.
13. according to arbitrary described charring process in claim 1 to 12, it is characterised in that：Lignin decomposes can be in nitrogen-ammonia
Carry out under body.
14. according to arbitrary described charring process in claim 1 to 13, it is characterised in that：Second crystallization can be at being about
210 °C to 215 °C.
15. according to arbitrary described charring process in claim 1 to 14, it is characterised in that：Sustainable 30 points are crystallized for the second time
Clock to 50 minutes.
16. according to arbitrary described charring process in claim 1 to 15, it is characterised in that：The step of water balance, can be at
About 81.1 kPa 0.8 (atm) is about 101.4 kPas (about 1 atm).
17. according to arbitrary described charring process in claim 14 to 16, it is characterised in that：Second crystallization includes continuing 30
The Slow cooling step of minute, described water balance step.
18. according to arbitrary described a kind of charring process based on cellulosic material in claim 14 to 17, it is characterised in that：
Second crystallization includes that one drops to about 20.3 kPas（0.2 atmospheric pressure）Drop of pressure process.
19. according to arbitrary described a kind of charring process based on cellulosic material in claim 14 to 18, it is characterised in that：
Second crystallization is carried out in a nitrogen environment.
20. according to arbitrary described a kind of charring process based on cellulosic material in claim 1 to 16, it is characterised in that：
Water balance step is carried out in about 95 DEG C.
21. according to arbitrary described a kind of charring process based on cellulosic material in claim 1 to 20, it is characterised in that：
Water balance step lasts about 60 minutes.
22. according to arbitrary described a kind of charring process based on cellulosic material in claim 1 to 21, it is characterised in that：
Water balance step is at about 50.7 kPas（About 0.5atm）In carry out.
23. according to arbitrary described a kind of charring process based on cellulosic material in claim 1 to 21, it is characterised in that：
Water balance step is at about 81.1 kPas（0.8 atm）To about 101.4 kPas（1 atm）In carry out.
24. according to arbitrary described a kind of charring process based on cellulosic material in claim 1 to 23, it is characterised in that：
Water balance step may be carried out in atmospheric humidity about 50%.
25. according to arbitrary described a kind of charring process based on cellulosic material in claim 1 to 21, it is characterised in that：
Charring process may further include gas and sour extraction step, before first time crystallizes.
A kind of 26. charring process based on cellulosic material according to claim 25, it is characterised in that：The gas and
Sour extraction step may be about 120 °C.
27. according to a kind of charring process based on cellulosic material described in claim 25 or 26, it is characterised in that：Gas
Sour extraction step is probably 90 minutes to 120 minutes.
28. according to arbitrary described a kind of charring process based on cellulosic material in claim 25 to 27, it is characterised in that：
Gas and sour extraction step may be about 101.4 kPas (about 1 atm).
29. according to arbitrary described a kind of charring process based on cellulosic material in claim 1 to 28, it is characterised in that：
Carbonization process may further include to constitute hemicellulose switch process, after second crystallizes.
30. according to a kind of charring process based on cellulosic material described in claim 29, it is characterised in that：Hemicellulose
Switch process may be about 195 °C.
31. according to a kind of charring process based on cellulosic material described in claim 29, it is characterised in that：Hemicellulose
Switch process may about 15 minutes.
32. according to a kind of charring process based on cellulosic material described in claim 29, it is characterised in that：Hemicellulose
Switch process may be about 101.4 kPas (about 1 atm).
33. according to arbitrary described a kind of charring process based on cellulosic material in claims 1 to 32, it is characterised in that：
Hemicellulose switch process can be carried out under nitrogen-ammonia gas.
34. according to arbitrary described a kind of charring process based on cellulosic material in claims 1 to 33, it is characterised in that：
Charring process may further include Slow cooling step after crystallizing at second, in about 1 minute under about 210 °C, about
91.3 kPas (0.9 atm).
35. according to arbitrary described a kind of charring process based on cellulosic material in claim 29 to 34, it is characterised in that：
The step of charring process may further include carbonization, which is after hemicellulose switch process.
36. according to a kind of charring process based on cellulosic material described in claim 35, it is characterised in that：Carbonization
120 °C may be about.
37. according to arbitrary described a kind of charring process based on cellulosic material in claim 35 to 36, it is characterised in that：
Carbonization is probably about 45 minutes.
38. according to arbitrary described a kind of charring process based on cellulosic material in claim 35 to 37, it is characterised in that：
Carbonization is probably about 101.4 kPas (about 1 atm).
39. according to arbitrary described a kind of charring process based on cellulosic material in claim 35 to 38, it is characterised in that：
Charring process may further include compacting step, and which is after carbonization.
40. according to a kind of charring process based on cellulosic material described in claim 39, it is characterised in that：Compacting step
180 °C may be about.
A kind of 41. charring process based on cellulosic material according to claim 39 or 40, it is characterised in that：Compacting step
Rapid is probably about 15 minutes.
42. according to arbitrary described a kind of charring process based on cellulosic material in claim 39 to 41, it is characterised in that：
Compacting step is probably about 91.3 kPas (0.9 atm).
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| US201462069921P | 2014-10-29 | 2014-10-29 | |
| US62/069,921 | 2014-10-29 | ||
| PCT/CA2015/051105 WO2016065477A1 (en) | 2014-10-29 | 2015-10-29 | Process for wood torrefaction, and construction material produced therefrom |
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| CN106573281B CN106573281B (en) | 2020-06-16 |
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| US11124461B2 (en) | 2019-07-04 | 2021-09-21 | Incitec Pivot Limited | Fertilizer |
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| WO2016065477A1 (en) | 2016-05-06 |
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